WO2018157160A1 - Systèmes d'implant nanostructuré à durée de vie améliorée et procédés - Google Patents

Systèmes d'implant nanostructuré à durée de vie améliorée et procédés Download PDF

Info

Publication number
WO2018157160A1
WO2018157160A1 PCT/US2018/020035 US2018020035W WO2018157160A1 WO 2018157160 A1 WO2018157160 A1 WO 2018157160A1 US 2018020035 W US2018020035 W US 2018020035W WO 2018157160 A1 WO2018157160 A1 WO 2018157160A1
Authority
WO
WIPO (PCT)
Prior art keywords
nanotube
coating
condition
medical device
contaminants
Prior art date
Application number
PCT/US2018/020035
Other languages
English (en)
Inventor
Sungho Jin
Daniel F. Justin
Original Assignee
Nanovation Partners LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanovation Partners LLC filed Critical Nanovation Partners LLC
Publication of WO2018157160A1 publication Critical patent/WO2018157160A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0035—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like
    • B08B7/0057—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by radiant energy, e.g. UV, laser, light beam or the like by ultraviolet radiation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
    • A61B90/00—Instruments, implements or accessories specially adapted for surgery or diagnosis and not covered by any of the groups A61B1/00 - A61B50/00, e.g. for luxation treatment or for protecting wound edges
    • A61B90/70—Cleaning devices specially adapted for surgical instruments
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
    • A61L2/14—Plasma, i.e. ionised gases
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02—Inorganic materials
    • A61L27/04—Metals or alloys
    • A61L27/06—Titanium or titanium alloys
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A61L31/082—Inorganic materials
    • A61L31/086—Phosphorus-containing materials, e.g. apatite
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/08—Materials for coatings
    • A61L31/082—Inorganic materials
    • A61L31/088—Other specific inorganic materials not covered by A61L31/084 or A61L31/086
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
    • A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L31/16—Biologically active materials, e.g. therapeutic substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B11/00—Cleaning flexible or delicate articles by methods or apparatus specially adapted thereto
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/041—Cleaning travelling work
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
    • B08B7/0064—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes
    • B08B7/0071—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by temperature changes by heating
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2/00—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor
    • A61L2/02—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using physical phenomena
    • A61L2/08—Radiation
    • A61L2/10—Ultraviolet radiation
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2202/00—Aspects relating to methods or apparatus for disinfecting or sterilising materials or objects
    • A61L2202/20—Targets to be treated
    • A61L2202/24—Medical instruments, e.g. endoscopes, catheters, sharps
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A61L2300/406—Antibiotics
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412—Tissue-regenerating or healing or proliferative agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2400/00—Materials characterised by their function or physical properties
    • A61L2400/18—Modification of implant surfaces in order to improve biocompatibility, cell growth, fixation of biomolecules, e.g. plasma treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B17/00—Methods preventing fouling
    • B08B17/02—Preventing deposition of fouling or of dust
    • B08B17/06—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement
    • B08B17/065—Preventing deposition of fouling or of dust by giving articles subject to fouling a special shape or arrangement the surface having a microscopic surface pattern to achieve the same effect as a lotus flower
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery

Definitions

  • the present disclosure relates to medical devices such as orthopedic implants, dental implants, in vitro biomedical implants, in vivo biomedical implants, cell growth devices, drug delivery devices, etc., all of which may benefit from an improved shelf life.
  • nanoscaled materials exhibit extraordinary electrical, optical, magnetic, chemical, and/or biological properties all of which may not be achieved via micro-scaled or bulk counterparts.
  • the development of nano-scaled materials has been intensively pursued in order to utilize such properties for various technical applications including biomedical and nano-bio applications.
  • nanoscale titanium oxide structures are set forth in: U .S. Patent Application Serial No. 1 1/913,062, filed June 10, 2008 and entitled "COMPOSITIONS COMPRISING NANOSTRUCTURES FOR CELL, TISSUE AND ARTIFICIAL ORGAN GROWTH, AND METHODS FOR MAKING AND USING SAME," now U .S. Patent No. 8,414,908; U.S. Patent Application Serial No.
  • Titanium (Ti) metal and Ti alloys such as Titanium-Aluminum-Vanadium (Ti-AI-V) are corrosion resistant, machinable, and light, yet sufficiently strong for load-bearing applications. They are one of the few biocompatible metals which osseo-integrate with bone material (e.g., by allowing direct chemical and/or physical bonding with adjacent bone surfaces without forming a fibrous tissue interface layer). For these reasons, Ti and Ti alloys have been used successfully in orthopedic and dental implants. See Handbook of biomaterial properties, edited by J. Black and G. Hasting, London; Chapman & Hall, 1998, and Biomaterials Science, a book by B. D. Ratner et al., San Diego, CA,: Academic press; 1996.
  • Ti Titanium Oxide
  • anatase phase is known to be better than the rutile phase of Ti02 (and other phases). See an article by Uchida et al, Journal of Biomedical Materials Research, Vol. 64, page 164-170 (2003).
  • Surface treatments such as roughening by sand blasting, formation of anatase phase ⁇ 02, hydroxyapatite coating, or other chemical treatments, have been utilized to further improve the bioactivity of the Ti surface and enhance bone growth.
  • Accelerated bone growth may be accomplished when the surface of Ti, or a Ti-6AI-4V alloy type implant, is anodized to form amorphous Ti02 nanotubes.
  • the Ti02 nanotube surface may then subsequently be annealed at 500°C to 550°C to crystallize the amorphous Ti02 nanotubes and form more desirable anatase type Ti02 nanotubes.
  • the Ti02 phase can be prepared by various techniques such as the sol-gel method, electrophoretic deposition, and anodization. See articles by. B.B. Lakshmi, et al., Chemistry of Materials, Vol. 9, page 2544-2550 (1997), Miao, et al., Nano Letters, Vol. 2, No.
  • anodized Ti02 nanotube arrays may exhibit highly hydrophilic properties which can be beneficial for good wetting properties and enhanced bone growth. Inadvertent accumulation of organic materials tends to reduce the hydrophilicity of anodized Ti02 nanotube arrays, which causes a shelf-life problem as the degree of such organic, or carbonaceous film, generally increases with time.
  • UV radiation ultraviolet
  • sterilization may be applied to the nanotube structures of implants or substrate materials having a variety of geometry and configurations.
  • sterilized and/or reactivated hydrophilic nanotube surface configurations may include ⁇ 02 nanotubes as well as oxide nanotube surfaces formed from alloys containing Ti or ⁇ 02 by at least 50% weight.
  • other related materials such as Zr, Hf, Nb, Ta, Mo, W, and their oxides, or alloys of these metals and oxides by at least 50% weight is also contemplated.
  • Si silicon, Si oxide, carbon, diamond, noble metals (such as Au, Ag, Pt and their alloys), polymer or plastic materials, or composite metals, ceramics or polymers can also be utilized to produce and use desired surface configurations for implant and cell growth applications.
  • noble metals such as Au, Ag, Pt and their alloys
  • polymer or plastic materials or composite metals, ceramics or polymers can also be utilized to produce and use desired surface configurations for implant and cell growth applications.
  • the coating may advantageously cover at least 70% of the total surface of the implant.
  • one or more plasma-based methods may be used to reactivate Ti-based nanotube structures and related implants by decomposing the organic or carbon type surface contaminants, such as hydrocarbon based and/or carbon-containing contaminants, at a much faster rate than would be obtained through the use of UV light.
  • Oxygen-based plasma, Argon-based plasma, Nitrogen-based plasma and/or other types of plasmas, and/or combinations/mixtures thereof may also be used, for example.
  • plasma treatment may enable relatively rapid reactivation of the bone in-growth properties of the nanotube coating.
  • heat-based methods may be used to remove organic film layers.
  • An implant with a nanotube coating as set forth above may be heated, for example, to a temperature of 400°C or less to reactivate the bone in-growth properties of the surface.
  • a method for removing contaminants from a medical device, that has a nanostructured surface may include commencing exposure of the nanostructured surface to at least one condition that at least partially removes the contaminants.
  • the at least one condition may be selected from: ultraviolet light, an elevated temperature, and/or a plasma.
  • the method may also include ceasing exposure of the nanostructured surface to the at least one condition after the contaminants are at least partially removed from the nanostructured surface.
  • the at least one condition may be applied to the nanostructured surface while it is in: a dry state, a wet state, and/or a protected state.
  • a method for removing contaminants from a medical device may include commencing exposure of the nanotube surface to at least one condition that at least partially removes the contaminants.
  • the at least one condition may be selected from: ultraviolet light, an elevated temperature, and/or a plasma.
  • the method may also include ceasing exposure of the nanotube surface to the at least one condition after the contaminants are at least partially removed from the nanotube surface, including the inner nanotube surfaces and the outer nanotube surfaces.
  • the nanotube surface may include an oxide nanotube coating formed from alloys containing at least one of Ti or Ti02 by at least 50% weight.
  • the oxide nanotube coating may include Ti02 anatase crystals.
  • the oxide nanotube coating may have a thickness of at least 30 nm.
  • the nanotube surface, and/or oxide nanotube coating may cover at least 70% of a total surface of the medical device.
  • a method for removing contaminants from a medical device may include providing a medical device that has a substrate and a nanotube surface covering at least a portion of a surface of the substrate.
  • the nanotube surface may include a plurality of nanotubes and the plurality of nanotubes may have a plurality of inner nanotube surfaces, a plurality of outer nanotube surfaces, and an oxide nanotube coating formed over the plurality of inner nanotube surfaces and outer nanotube surfaces.
  • the method may also include commencing exposure of the nanotube surface to at least one condition that at least partially removes the contaminants.
  • the at least one condition may be selected from: ultraviolet light, an elevated temperature, and/or a plasma.
  • the method may also include ceasing exposure of the nanotube surface to the at least one condition after the contaminants are at least partially removed from the nanotube surface, including the inner nanotube surfaces and the outer nanotube surfaces.
  • the oxide nanotube coating may be formed from alloys containing at least one of Ti or Ti02 by at least 50% weight.
  • the oxide nanotube coating may include Ti02 anatase crystals.
  • the oxide nanotube coating may have a thickness of at least 30 nm.
  • the nanotube surface, and/or oxide nanotube coating may cover at least 70% of a total surface of the medical device.
  • a medical device may include surface nanotubes made from oxides having at least one of: Ti, Zr, V, Ta, Nb, Hf, Mo, and/or W.
  • the surface nanotubes of the medical device may exhibit an increase in hydrophilicity after exposure to at least one condition that at least partially removes contaminants from the surface nanotubes of the medical device.
  • the at least one condition may be selected from: ultraviolet light, an elevated temperature, and/or a plasma.
  • the surface nanotubes of the medical device may substantially maintain their increased super-hydrophilic properties after undergoing a storage period of at least three months within a protected environment.
  • FIG. 1 A illustrates a cross-sectional side view of a medical device that incorporates a nanotube surface
  • FIGS. 1 B-D illustrate how a water droplet may interact with the nanotube surface of FIG. 1A according to the presence (or absence) of organic contaminants on the nanotube surface;
  • FIG. 2A illustrates the nanotube surface of FIG. 1A with organic matter contaminants on the nanotube surface
  • FIGS. 2B-2D depict various ways of treating the nanotube surface of FIG. 1 A with UV radiation to remove the organic matter contaminants
  • FIGS. 3A and 3B illustrate exemplary UV lamp configurations that are suitable for treating the nanotube surface of FIG. 1A;
  • FIG. 4 illustrates a thermal-based method of treating a nanotube surface to re-activate an aged or contaminated nanotube surface
  • FIGS. 5A and 5B illustrate plasma-based methods of treating a nanotube surface to achieve rapid decomposition of organic contaminants from the nanotube surface of FIG. 1 A;
  • FIG. 6 illustrates a method of treating a nanotube surface to remove organic contaminants.
  • Implants with a ⁇ 02 nanotube surface may be different from regular Ti implants in that the Ti02 coated nanotube surface includes vertically aligned, small-diameter (e.g., 30 to 300 nm diameter) and relatively tall (e.g., 100 - 2,000 nm height), tube-like nanostructures.
  • Ti02 nanotube surfaces may be particularly susceptible to surface contamination due to the higher reactivity of their nanoscale surfaces. Possible contaminants that may interact with the nanoscale surface may include, but are not limited to: oily matter, organic material, hydrocarbon based material, nitrogen-based material, sulfide-based material, and the like. These contaminants may slowly accumulate on the nanotube surface over an extended period of time (e.g., seconds, minutes, hours, days, months, years, etc.).
  • a shelf-aged Ti or Ti02 nanotube surface may lose its original super-hydrophilic characteristic, which is an important characteristic for the adhesion and growth of osteoblast cells, protein molecules, hydroxyapatite components, and the like. Moreover, longer exposure times typically result in more extensive contamination of the nanotube surface, resulting in a more severe loss of hydrophilicity. Accordingly, the shelf life characteristics of implantable materials is an important issue that must be addressed.
  • any of three approaches may be used to re-activate a Ti02 coated nanotube surface (and/or other refractive metal oxide nanotubes as well), by decomposing and/or removing the oily matter, organic material, and/or hydrocarbon-based contaminants from the nanotube surface.
  • These three approaches may include, but are not limited to: (1 ) UV exposure of the Ti02 nanotube surface; (2) Re-activation thermal annealing at low temperature without introducing thermal stress and/or micro-cracking; and (3) More rapid re-activation of Ti02 nanotube surface by using plasma bathing including, but not limited to: oxygen plasma, argon plasma, nitrogen plasma, and/or other suitable plasmas.
  • High-aspect ratio nanotubes may be difficult to clean and re-activate because the size and shape of high-aspect ratio nanotubes may naturally interfere with the above cleaning/re-activation processes.
  • the size and shape of high-aspect ratio nanotubes may make it more difficult to shine UV light into the interior of the nanotubes to sufficiently clean/reactivate the interior and/or exterior surfaces of the nanotubes. Accordingly, the present disclosure describes improved reactivation methods which may be particularly useful for implants that incorporate high-aspect-ratio nanotube structures.
  • FIG. 1 A illustrates a cross-sectional side view of a medical device 10, or substrate 10, incorporating a nanostructured surface (or nanotube surface) 20 covering at least a partial surface of the medical device/substrate 10.
  • the nanostructured surface 20 may be made predominantly of a plurality of nanotubes (1-10).
  • ten nanotubes (1 -10) are shown for the purposes of illustrating the general concepts disclosed herein. However, it will be understood that any number nanotubes are contemplated without departing from the spirit or scope of the present disclosure.
  • FIG. 1 A illustrates a cross-sectional side view of a medical device 10, or substrate 10, incorporating a nanostructured surface (or nanotube surface) 20 covering at least a partial surface of the medical device/substrate 10.
  • the nanostructured surface 20 may be made predominantly of a plurality of nanotubes (1-10).
  • ten nanotubes (1 -10) are shown for the purposes of illustrating the general concepts disclosed herein. However, it will be understood that any number nanotubes are
  • the ten nanotubes (1-10) shown each have inner bores 30 that define a plurality of inner nanotube surfaces 31 lying within the interior regions of the inner bores 30, as well as a plurality of outer nanotube surfaces 32 outside of the inner bores 30 of the nanotubes (1 -10).
  • the nanostructured surface 20 may also include micro-scale surface features and/or imperfections (not shown).
  • the nanostructured surface 20 may further include at least one characteristic selected from: randomly structured nanopores, randomly structured nanorods, periodic structured nanopores, and/or periodic structured nanorods.
  • the nanotube surface 20 may be anodized with a coating of Ti02 nanotubes (1 -10), which may then undergo an additional annealing process, and/or be packaged and stored according to techniques known in the art.
  • the ⁇ 02 coated nanotube surface 20 may incorporate high-aspect-ratio nanotube structures (1 -10) that: (1 ) may be substantially vertically aligned; (2) may have small-diameters (e.g., 30 nm to 300 nm); (3) may be relatively tall (e.g., 100 nm - 2,000 nm in height;
  • the high-aspect-ratio nanotube structures (1 -10) may have nanotube heights of less than 10 urn); and/or (4) may have nanotube lateral dimensions less than 1 ,000 nm (In some embodiments, the high-aspect-ratio nanotube structures (1 -10) may have nanotube lateral dimensions of less than 400 nm).
  • the nanotube surface 20 may include an oxide nanotube coating formed from alloys containing at least one of Ti or Ti02 by at least 50% weight.
  • the nanotube surface 20 may include an oxide nanotube coating formed from alloys containing at least one of Zr, V, Ta, Nb, Hf, Mo, W, or their oxides, by at least 50% weight.
  • the oxide nanotube coating may include Ti02 anatase crystals.
  • the oxide nanotube coating may have a thickness of at least 30 nm.
  • the oxide nanotube coating may cover at least 70% of a total surface of the medical device.
  • the nanostructured surface 20 may also include at least one coating selected from: (1) a coating that includes hydroxyapatite with a thickness of at least 2 nm; (2) a coating that includes calcium; (3) a coating that includes potassium; (4) a coating that includes Ta; (5) a coating that includes Ta-oxide; (6) a coating that includes at least one biological agent and the coating is at least partially present on the plurality of inner nanotube surfaces 31 ; (7) a coating that includes at least one catalyst and the coating is at least partially present on the plurality of inner nanotube surfaces 31 ; (8) a coating that includes at least one catalyst and the coating is at least partially present on the plurality of inner nanotube surfaces 31 ; (9) a coating that includes at least one cell-growth-stimulating agent and the coating is at least partially present on the plurality of inner nanotube surfaces 31 ; (10) a coating that includes at least one antibiotic and the coating is at least partially present on the plurality of inner nanotube surfaces 31 ; and/or (1 1) any coating selected from: (1) a coating
  • FIGS. 1 B-D illustrate how a water droplet 40 may interact with the nanotube surface 20 of the medical device 10 of FIG. 1A according to the presence, or absence, of organic contaminants on the nanotube surface 20. More specifically, FIGS. 1 B-D illustrate the hydrophobic/hydrophilic properties of the nanotube surface 20 and how a contact angle ⁇ associated with the water droplet 40 placed on top of the nanotube surface 20 may vary due to the presence, or absence, of organic contaminants on the nanotube surface 20, thus affecting the hydrophobic/hydrophilic characteristics of the nanotube surface 20.
  • FIG. 1 B depicts virgin/clean nanotubes on the surface of the medical device 10 of FIG. 1A. Since there are no (or at least very little) organic matter contaminants present on the nanotube surface 20 of the medical device 10 in FIG. 1 B, the nanotube surface 20 retains its super-hydrophilic characteristics and readily absorbs the water droplet 40 into the nanotube structures, as is shown in FIG. 1 B.
  • the water droplet 40 shown in FIG. 1 B may have a contact angle ⁇ of about 0 to 10 degrees.
  • FIG. 1 C depicts the medical device 10 of FIG. 1 B after the nanotubes have become contaminated with organic matter. Since organic matter contaminants are present on the nanotube surface 20 of the medical device 10 in FIG. 1 C, the nanotube surface 20 adopts a more hydrophobic characteristic which tends to repel the water droplet 40, preventing absorption of the water droplet 40 into the nanotube structures, as is shown in FIG. 1 C.
  • the water droplet 40 shown in FIG. 1 B may have a contact angle ⁇ of about 10 to 100 degrees.
  • FIG. 1 D depicts the medical device 10 of FIG. 1 C after the nanotubes have been processed by cleaning techniques disclosed herein to remove, or at least partially remove, the organic matter contaminants and restore the hydrophilic characteristics of the nanotubes, such that the nanotube surface 20 may once again readily absorb the water droplet 40 into the nanotube structures.
  • the water droplet 40 shown in FIG. 1 B may once again have a contact angle ⁇ of about 0 to 10 degrees.
  • FIGS. 1 B-D illustrate how the desired hydrophilicity of the nanotube surface 20 may be lost over time due to the time-dependent accumulation of organic, oily, hydrocarbon based, and/or carbon- containing contaminants through exposure to the air environment, or other materials, and how this hydrophilicity may then be recovered by cleaning processes described herein.
  • the cleaning processes described herein may include commencing exposure of the nanotube surface 20, including the inner nanotube surfaces 31 and the outer nanotube surfaces 32, to at least one condition that at least partially removes the contaminants from the nanotube surface 20.
  • the at least one condition may generally be selected from: ultraviolet light, an elevated temperature, and plasma. Once the at least one condition has at least partially removed from the contaminants from the nanotube surface 20, including the inner nanotube surfaces 31 and the outer nanotube surfaces 32, exposure of the nanotube surface 20 to the at least one condition may be ceased.
  • FIGS. 2B-2D depict various ways of treating the nanotube surface 20 of FIG. 2A with UV radiation 50 to remove these organic matter contaminants 35 while the nanotube surface 20 is in various states including, but not limited to: a dry state, a wet state, and a protected state.
  • Example UV radiation characteristics may include, for example, UV light wavelengths between about 260 nm to 350 nm with 10 to 100 watts of power and about 0.05 to 10 mW/cm 2 intensity.
  • FIG. 2B illustrates the use of UV radiation 50 to remove the organic matter contaminants 35 from the nanotubes while the medical device 10 is in a "dry state” by shining UV radiation 50 down into the inner bores 30 of the nanotubes to remove organic matter contaminants 35 from the inner nanotube surfaces 31 of the nanotubes, as well as remove organic matter contaminants 35 from the outer nanotube surfaces 32 of the nanotubes.
  • a “dry state” may be defined as a state in which the medical device 10 is substantially free from liquids.
  • FIG. 2C illustrates the use of UV radiation 50 to remove the organic matter contaminants 35 from the nanotubes while the medical device 10 is in a "wet state" by shining UV radiation 50 down into the inner bores 30 of the nanotubes to remove organic matter contaminants 35 from the inner nanotube surfaces 31 of the nanotubes, as well as remove organic matter contaminants 35 from the outer nanotube surfaces 32 of the nanotubes.
  • a "wet state” may be defined as a state in which the medical device 10 is in contact with one or more liquids.
  • the medical device 10 may be placed in a container 60 and submerged, or at least partially submerged, in a liquid 70, such as a suitable cleaning solution, aqueous solution, solvent, alcohol solution, or other suitable liquid 70, while at the same time undergoing exposure to UV radiation 50.
  • a suitable liquid 70 may speed up and/or otherwise facilitate the UV radiation 50 cleaning process.
  • FIG. 2D illustrates the use of UV radiation 50 to remove organic matter contaminants 35 from the nanotubes while the medical device 10 is in a "protected state" by shining UV radiation 50 down into the inner bores 30 of the nanotubes to remove organic matter contaminants 35 from the inner nanotube surfaces
  • a "protected state” may be defined as a state in which the medical device 10 is encapsulated, or at least partially encapsulated, within a protective barrier 80 which separates, or at least partially separates, the medical device 10 from its surrounding environment.
  • a medical device may be placed within a suitable medical device package (not shown) which may substantially prevent, or at least slow down, the passage of ambient air and contaminants through the medical device packaging in order to protect the medical device from becoming contaminated by the outside environment.
  • a suitable medical device package may also be pre-filled with a sterile/inert gas (e.g., Ar, N2, and the like) to help further protect a medical device 10 placed therein.
  • a sterile/inert gas e.g., Ar, N2, and the like
  • the interior of the medical device package may also be placed under a vacuum to help protect a medical device 10 placed therein.
  • the protective barrier 80 may also be made of materials that readily allow the passage of UV radiation 50 through the protective barrier 80, while at the same time substantially preventing, or at least slowing down, the passage of ambient air and contaminants through the protective barrier 80.
  • the protective barrier 80 may be made from a UV-transparent plastic, glass, quartz, or other material which readily allows the passage of UV radiation 50 through the protective barrier 80, while substantially preventing, or at least slowing down, the passage of contaminants and/or other matter through the protective barrier 80.
  • FIGS. 3A and 3B illustrate exemplary UV radiation configurations that may be used to treat the nanotube surfaces of medical devices disclosed herein.
  • FIGS. 3A and 3B illustrate exemplary UV radiation configurations that may be used to enhance the UV radiation treatment of medical devices 10 that incorporate high-aspect-ratio Ti02 nanotube surfaces 20 with nanotubes which may be vertically aligned, have small-diameters (e.g., 30 to 300 nm diameters), and may be relatively tall (e.g., 100 nm - 2,000 nm in height).
  • These characteristics of high-aspect-ratio Ti02 nanotubes may make it difficult for UV radiation to illuminate all of, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 of the nanotubes to substantially remove any organic contaminants thereon.
  • FIG. 3A illustrates a medical device 10 enclosed within a chamber (or oven) 95 that is being exposed to UV radiation 50 emitted from at least one UV light source, such as a UV lamp 90.
  • the UV lamp 90 may be rotated and/or translated relative to the medical device 10 in order to orient the UV lamp 90 in a plurality of different orientations relative to the nanotube surface 20.
  • the UV radiation 50 emitted from the UV lamp 90 may substantially illuminate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 to enhance removal of the contaminants.
  • This process may be especially beneficial for medical devices 10 with complicated 3D geometries in order to provide UV exposure to all of the surfaces of the medical device 10.
  • the chamber (or oven) 95 may also be filled with any suitable gas, such as ambient air, N2, Ar, and the like.
  • FIG. 3B illustrates the medical device 10 of FIG. 3A enclosed within the chamber (or oven) 95 and undergoing exposed to UV radiation 50 emitted from the UV lamp 90.
  • the medical device 10 may be rotated and/or translated relative to the UV lamp 90 in order to orient the nanotube surface 20 of the medical device 10 in a plurality of different orientations relative to the U V lamp 90.
  • the UV radiation 50 emitted from the UV lamp 90 may substantially illuminate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 to enhance removal of the contaminants.
  • both the UV lamp 90 and the medical device 10 may be rotated and/or translated relative to each other at the same time in order to orient the nanotube surface 20 of the medical device 10 in a plurality of different orientations relative to the UV lamp 90, such that the UV radiation 50 emitted from the UV lamp 90 may substantially illuminate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 and enhance removal of the contaminants.
  • FIG. 4 illustrates a thermal-based method of treating a nanotube surface 20 to re-activate an aged or contaminated nanotube surface 20. For example, heating-based removal of an organic film layer or other carbonaceous layer accumulated can be performed on the ⁇ 02 nanotube surfaces 20 previously discussed herein .
  • ⁇ 02 nanotube surfaces 20 may undergo an additional crystallization annealing process through exposure to a crystallization annealing temperature, after an anodization process has been performed, in order to form the more desirable anatase phase of ⁇ 02.
  • This crystallization annealing temperature may generally be performed at a temperature (Ti) of about 500°C to 550°C, as shown in FIG. 4.
  • the heating temperature for removal of organic contaminants from the Ti02 nanotube surfaces 20 may advantageously be set at a lower temperature (T 2 ), such as about 400°C or lower, so as to minimize thermal cycling induced by Coefficient of Thermal Expansion (CTE) mismatch between different materials and associated weakening of the interface between the Ti matrix and Ti02 nanotube layer.
  • T 2 a lower temperature
  • This nanotube re-activation heat treatment process may advantageously also be used with limited frequency so as to avoid fatigue-based micro-cracking and/or delamination of the Ti02 nanotube layer from the Ti (or Ti-AI-V based alloy, etc.).
  • a medical device 10 may be exposed to an elevated temperature that is below a crystallization anneal temperature of a nanotube surface associated with the medical device 10.
  • the maximum temperature may be limited to 400°C or less.
  • any suitable temperature above 400°C and/or below 400°C may also be used, depending on the specific materials and/or construction of the medical device 10 undergoing heat- based treatment. Relatively slow heating and/or cooling rates may also be used during heat-based treatment in order to further minimize thermal stresses to the medical device 10.
  • heat-based treatment may also be combined with any other treatment or method disclosed herein.
  • FIGS. 5A and 5B illustrate plasma-based methods of treating a nanotube surface of a medical device in order to achieve rapid decomposition of organic contaminants from the nanotube surface of the medical device.
  • FIG. 5A shows a medical device 10 that is placed within a plasma chamber 500 and exposed to a plasma 520.
  • Plasma 520 may breakdown organic or carbon containing contaminants in a relatively short period of time (e.g., usually minutes rather than hours). This method may be desirable for achieving high- throughput re-activation of hydrophilic ⁇ 02 nanotube surfaces.
  • Suitable plasmas for this process may include, but are not limited to: oxygen-based plasma, argon-based plasma, nitrogen-based plasma, and the like.
  • FIG. 5B shows the medical device 10 of FIG. 5A enclosed within the plasma chamber 500 and undergoing exposure to the plasma 520.
  • the medical device 10 may also be rotated and/or translated within the plasma chamber 500 relative to the plasma 520 within the chamber 500 in order to orient the nanotube surface 20 of the medical device 10 in a plurality of different orientations relative to the plasma 520.
  • the plasma 520 may more quickly and/or more substantially infiltrate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 to enhance removal of the contaminants.
  • the plasma 520 within the chamber 500 may itself be rotated and/or translated within the plasma chamber 500 relative to the medical device 10 in order to further orient the nanotube surface 20 of the medical device 10 in a plurality of different orientations relative to the plasma 520. In this manner, the plasma 520 may more quickly and/or more substantially infiltrate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 to enhance removal of the contaminants by the plasma 520.
  • both the plasma 520 and the medical device may be rotated and/or translated within the plasma chamber 500 relative to each other at the same time in order to orient the nanotube surface 20 of the medical device 10 in a plurality of different orientations relative to the plasma 520 and allow the plasma 520 to more quickly and/or more substantially infiltrate all, or at least a substantial portion of, the inner nanotube surfaces 31 and the outer nanotube surfaces 32 to enhance removal of the contaminants by the plasma 520.
  • a medical device 10 may include surface nanotubes 20 made from oxides having at least one of: Ti, Zr, V, Ta, Nb, Hf, Mo, and/or W.
  • the surface nanotubes 20 of the medical device 10 may exhibit an increase in its super-hydrophilic properties after exposure to at least one condition that at least partially removes contaminants from the surface nanotubes 20 of the medical device 10.
  • the at least one condition may be selected from: ultraviolet light, an elevated temperature (e.g. 500°C or less), and/or a plasma.
  • the surface nanotubes 20 of the medical device 10 may substantially maintain their increased super-hydrophilic properties after undergoing a storage period of at least three months within a protected environment.
  • the protected environment may include at least one of: a protective gas environment, a sealed environment, a vacuum-sealed environment, a plastic-wrapped environment, a metal-foil-wrapped environment, and the like.
  • the super-hydrophilic properties of the surface nanotubes 20 may be further verified after the medical devices has completed the storage period of at least three months within the protected environment.
  • the super-hydrophilic properties of the surface nanotubes 20 may be verified by performing a water droplet contact angle test whereupon the surface nanotubes 20 may exhibit a water droplet contact angle of less than about 5 degrees, in one non-limiting example.
  • the surface nanotubes 20 may exhibit a water droplet contact angle of less than about 2 degrees.
  • the surface nanotubes 20 may exhibit a water droplet contact angle of about 5 to 20 degrees.
  • FIG. 6 illustrates a method 600 of treating a nanotube surface 20 in order to remove organic contaminants.
  • the method 600 may include any of the treatments disclosed herein including: UV radiation exposure, heat-based treatments, plasma-based treatments, and/or any combinations thereof.
  • the method 600 may begin with a step 610 in which a medical device 10 comprising a nanotube surface 20 may be provided. Any type of medical device 10 disclosed herein may be provided and the medical device 10 that is provided may further include any type of nanotube surface 20 described herein.
  • the method 600 may then proceed to a step 620 in which the nanotube surface 20 of the medical device 10 may be exposed to at least one condition that at least partially removes contaminants from the nanotube surface 20 of the medical device 10.
  • the method 600 may include any of the treatments disclosed herein including: UV radiation exposure, heat-based treatments, plasma-based treatments, and combinations thereof.
  • the method 600 may then proceed through one or more of the following steps (630, 640, 650, 660, and 670) of the method 600. However, it will be understood that these steps are not required.
  • the method 600 may proceed to a step 630 in which the nanotube surface 20 may be oriented relative to the at least one condition to enhance removal of the contaminants by exposure to the at least one condition. This may be accomplished by additionally proceeding through one or more of steps 640, 650, 660, and 670 of the method 600.
  • the method 600 may proceed to a step 640 in which the nanotube surface 20 may be oriented relative to the at least one condition by rotating the nanotube surface 20 relative to the at least one condition.
  • the at least one condition including: UV radiation, heat, plasma, and/or combinations thereof.
  • the method 600 may alternatively, or in addition thereto, proceed to a step 650 in which the nanotube surface 20 may be oriented relative to the at least one condition by translating the nanotube surface 20 relative to the at least one condition.
  • the method 600 may alternatively, or in addition thereto, proceed to a step 660 in which the at least one condition may be oriented relative to nanotube surface 20 by rotating the at least one condition relative to the nanotube surface 20.
  • the at least one condition may include UV radiation exposure, heat-based treatments, plasma-based treatments, and/or combinations thereof.
  • the method 600 may alternatively, or in addition thereto, proceed to a step 670 in which the at least one condition may be oriented relative to nanotube surface 20 by translating the at least one condition relative to the nanotube surface 20.
  • the method 600 may proceed to a step 680 in which exposure of the nanotube surface 20 of the medical device 10 to the at least one condition may be ceased after the contaminants have been at least partially removed from the nanotube surface 20, and the method 600 my end.
  • any methods disclosed herein comprise one or more steps or actions for performing the described method.
  • the method steps and/or actions may be interchanged with one another.
  • the order and/or use of specific steps and/or actions may be modified.
  • phrases “connected to,” “coupled to” and “in communication with” refer to any form of interaction between two or more entities, including mechanical, electrical, magnetic, electromagnetic, fluid, and thermal interaction. Two components may be functionally coupled to each other even though they are not in direct contact with each other.
  • the term “abutting” refers to items that are in direct physical contact with each other, although the items may not necessarily be attached together.
  • the phrase “fluid communication” refers to two features that are connected such that a fluid within one feature is able to pass into the other feature.

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Epidemiology (AREA)
  • Surgery (AREA)
  • Heart & Thoracic Surgery (AREA)
  • Inorganic Chemistry (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Medicinal Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Vascular Medicine (AREA)
  • Transplantation (AREA)
  • Dermatology (AREA)
  • Physics & Mathematics (AREA)
  • Molecular Biology (AREA)
  • Biomedical Technology (AREA)
  • Optics & Photonics (AREA)
  • Medical Informatics (AREA)
  • Pathology (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Plasma & Fusion (AREA)
  • Materials For Medical Uses (AREA)

Abstract

L'invention concerne des procédés et des traitements pour éliminer des contaminants de surfaces de nanotubes recouvrant un dispositif médical. Ces procédés et traitements consistent à commencer l'exposition d'une surface de nanotube à au moins une condition qui élimine au moins partiellement les contaminants, comprenant : une lumière ultraviolette, une température élevée, un plasma et/ou des combinaisons de ceux-ci. Ces procédés et traitements peuvent également comprendre l'orientation de la surface de nanotube par rapport à la ou aux conditions afin d'améliorer l'élimination des contaminants par la ou les conditions. L'exposition de la surface de nanotube à la ou aux conditions peut être interrompue après que les contaminants aient été au moins partiellement éliminés de la surface de nanotube.
PCT/US2018/020035 2017-02-27 2018-02-27 Systèmes d'implant nanostructuré à durée de vie améliorée et procédés WO2018157160A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201762464268P 2017-02-27 2017-02-27
US62/464,268 2017-02-27

Publications (1)

Publication Number Publication Date
WO2018157160A1 true WO2018157160A1 (fr) 2018-08-30

Family

ID=63245934

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2018/020035 WO2018157160A1 (fr) 2017-02-27 2018-02-27 Systèmes d'implant nanostructuré à durée de vie améliorée et procédés

Country Status (2)

Country Link
US (1) US10857575B2 (fr)
WO (1) WO2018157160A1 (fr)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10857575B2 (en) 2017-02-27 2020-12-08 Nanovation Partners LLC Shelf-life-improved nanostructured implant systems and methods
US11559375B2 (en) * 2020-07-16 2023-01-24 Leszek Aleksander Tomasik Diamond dental teeth formed by using laser energy

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020159917A1 (en) * 2001-04-27 2002-10-31 Swart Sally Kay System and method for cleaning, high level disinfection, or sterilization of medical or dental instruments or devices
US20020198601A1 (en) * 2001-06-21 2002-12-26 Syntheon, Llc Method for microporous surface modification of implantable metallic medical articles and implantable metallic medical articles having such modified surface
US20050252805A1 (en) * 2004-05-11 2005-11-17 Cervantes Marvin J Protective packaging assembly for medical devices and method of using same
WO2006043166A2 (fr) * 2004-10-22 2006-04-27 Guya Bioscience S.R.L. Procede de preparation d'implants intraosseux presentant un haut degre d'integration osseuse par formation d'une couche mince de dioxyde de titane de structure cristalline anatase
US20090250588A1 (en) * 2006-01-04 2009-10-08 Liquidia Technologies, Inc. Nanostructured Surfaces for Biomedical/Biomaterial Applications and Processes Thereof
US20110116967A1 (en) * 2007-11-21 2011-05-19 University Of Florida Research Foundation Inc. Self-sterilizing device using plasma fields
US20120288699A1 (en) * 2011-05-11 2012-11-15 Ahlberg Elisabet Biocompatible component
US20130323119A1 (en) * 2012-06-01 2013-12-05 Carefusion 303, Inc. System and method for disinfection of medical devices
US20170007743A1 (en) * 2014-03-26 2017-01-12 Nanovis, LLC Anti-microbial device and method for its manufacture

Family Cites Families (82)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6250984B1 (en) 1999-01-25 2001-06-26 Agere Systems Guardian Corp. Article comprising enhanced nanotube emitter structure and process for fabricating article
US6283812B1 (en) 1999-01-25 2001-09-04 Agere Systems Guardian Corp. Process for fabricating article comprising aligned truncated carbon nanotubes
US6538367B1 (en) 1999-07-15 2003-03-25 Agere Systems Inc. Field emitting device comprising field-concentrating nanoconductor assembly and method for making the same
US6322713B1 (en) 1999-07-15 2001-11-27 Agere Systems Guardian Corp. Nanoscale conductive connectors and method for making same
US6504292B1 (en) 1999-07-15 2003-01-07 Agere Systems Inc. Field emitting device comprising metallized nanostructures and method for making the same
US6465132B1 (en) 1999-07-22 2002-10-15 Agere Systems Guardian Corp. Article comprising small diameter nanowires and method for making the same
US6286226B1 (en) 1999-09-24 2001-09-11 Agere Systems Guardian Corp. Tactile sensor comprising nanowires and method for making the same
US6340822B1 (en) 1999-10-05 2002-01-22 Agere Systems Guardian Corp. Article comprising vertically nano-interconnected circuit devices and method for making the same
US6741019B1 (en) 1999-10-18 2004-05-25 Agere Systems, Inc. Article comprising aligned nanowires
CA2322714A1 (fr) 1999-10-25 2001-04-25 Ainissa G. Ramirez Article compose d'alliages de metaux nobles ameliores et methode de fabrication connexe
US6297063B1 (en) 1999-10-25 2001-10-02 Agere Systems Guardian Corp. In-situ nano-interconnected circuit devices and method for making the same
EP1129990A1 (fr) 2000-02-25 2001-09-05 Lucent Technologies Inc. Procédé de croissance contrôlée de nanotubes de carbone
US6297592B1 (en) 2000-08-04 2001-10-02 Lucent Technologies Inc. Microwave vacuum tube device employing grid-modulated cold cathode source having nanotube emitters
JP2002141633A (ja) 2000-10-25 2002-05-17 Lucent Technol Inc 垂直にナノ相互接続された回路デバイスからなる製品及びその製造方法
GB0120993D0 (en) * 2001-08-30 2001-10-24 Quay Technologies Pulsed UV light source
EP1429683B1 (fr) * 2001-09-28 2014-12-24 Boston Scientific Limited Dispositifs medicaux contenant des nanomateriaux, et methodes therapeutiques faisant appel auxdits dispositifs
US20030133637A1 (en) 2002-01-16 2003-07-17 Zhenan Bao Lithium niobate waveguide device incorporating Li-trapping layers
US6900421B2 (en) * 2002-02-08 2005-05-31 Ecofriend Technologies, Inc. Microwave-assisted steam sterilization of dental and surgical instruments
US6809465B2 (en) 2002-08-23 2004-10-26 Samsung Electronics Co., Ltd. Article comprising MEMS-based two-dimensional e-beam sources and method for making the same
US6858521B2 (en) 2002-12-31 2005-02-22 Samsung Electronics Co., Ltd. Method for fabricating spaced-apart nanostructures
WO2004032275A2 (fr) 2002-08-23 2004-04-15 The Regents Fo The University Of California Dispositif de microtube a vide sur puce ameliore et procede de fabrication
WO2005004196A2 (fr) 2002-08-23 2005-01-13 Sungho Jin Article renfermant des structures a emission de champ a grille comprenant des nanofils centralises et procede de fabrication correspondant
US7233101B2 (en) 2002-12-31 2007-06-19 Samsung Electronics Co., Ltd. Substrate-supported array having steerable nanowires elements use in electron emitting devices
US7012266B2 (en) 2002-08-23 2006-03-14 Samsung Electronics Co., Ltd. MEMS-based two-dimensional e-beam nano lithography device and method for making the same
US6987027B2 (en) 2002-08-23 2006-01-17 The Regents Of The University Of California Microscale vacuum tube device and method for making same
US20050079282A1 (en) 2002-09-30 2005-04-14 Sungho Jin Ultra-high-density magnetic recording media and methods for making the same
US20040071951A1 (en) 2002-09-30 2004-04-15 Sungho Jin Ultra-high-density information storage media and methods for making the same
US7068582B2 (en) 2002-09-30 2006-06-27 The Regents Of The University Of California Read head for ultra-high-density information storage media and method for making the same
WO2004099469A2 (fr) 2003-04-09 2004-11-18 The Regents Of The University Of California Lithographie electrolytique haute resolution, dispositif associe et produits obtenus
WO2005065281A2 (fr) 2003-12-31 2005-07-21 The Regents Of The University Of California Articles comprenant un materiau nanocomposite a conductivite electrique elevee et procede permettant de produire ces articles
US7344685B2 (en) * 2004-01-17 2008-03-18 Mcnulty James F Ozonizer apparatus employing a multi-compartment bag for sterilizing
US7465210B2 (en) 2004-02-25 2008-12-16 The Regents Of The University Of California Method of fabricating carbide and nitride nano electron emitters
US7276389B2 (en) 2004-02-25 2007-10-02 Samsung Electronics Co., Ltd. Article comprising metal oxide nanostructures and method for fabricating such nanostructures
US20050238810A1 (en) * 2004-04-26 2005-10-27 Mainstream Engineering Corp. Nanotube/metal substrate composites and methods for producing such composites
WO2006135375A2 (fr) 2004-07-21 2006-12-21 The Regents Of The University Of California Nanostructure a courbe nanometrique de croissance catalytique et son procede de fabrication
US20080020499A1 (en) 2004-09-10 2008-01-24 Dong-Wook Kim Nanotube assembly including protective layer and method for making the same
US20060057388A1 (en) 2004-09-10 2006-03-16 Sungho Jin Aligned and open-ended nanotube structure and method for making the same
US8333948B2 (en) 2004-10-06 2012-12-18 The Regents Of The University Of California Carbon nanotube for fuel cell, nanocomposite comprising the same, method for making the same, and fuel cell using the same
US7868850B2 (en) 2004-10-06 2011-01-11 Samsung Electronics Co., Ltd. Field emitter array with split gates and method for operating the same
WO2006041691A2 (fr) 2004-10-06 2006-04-20 The Regents Of The University Of California Structure de nanosonde a base de nanotubes amelioree et procede de fabrication associe
GB0426346D0 (en) * 2004-12-01 2005-01-05 Csma Ltd Cleaning method
US7576341B2 (en) 2004-12-08 2009-08-18 Samsung Electronics Co., Ltd. Lithography systems and methods for operating the same
WO2006078952A1 (fr) 2005-01-21 2006-07-27 University Of California Procedes de fabrication d'un reseau periodique ordonne a longue portee de nano-elements, et articles comprenant ce reseau
WO2006116752A2 (fr) * 2005-04-28 2006-11-02 The Regents Of The University Of California Compositions comprenant des nanostructures destinées à la croissance de cellules, de tissus et d'organes artificiels, procédés de préparation et d'utilisation de ces dernières
WO2007081381A2 (fr) 2005-05-10 2007-07-19 The Regents Of The University Of California Nanostructures a motifs spinodaux
WO2007078316A2 (fr) 2005-05-10 2007-07-12 The Regents Of The University Of California Structures de sondes effilees et leur fabrication
EP1909852A4 (fr) 2005-06-16 2009-02-18 Univ California Structure des canaux des proteiques beta amyloide et utilisations de celle-ci dans l'identification de molecules de medicaments potentielles destinees a des maladies neurodegeneratives
WO2007047337A2 (fr) 2005-10-13 2007-04-26 The Regents Of The University Of California Systeme de sonde ameliore comprenant une pointe a alignement par champ electrique et procede de fabrication de ce systeme
US9149564B2 (en) 2006-06-23 2015-10-06 The Regents Of The University Of California Articles comprising large-surface-area bio-compatible materials and methods for making and using them
WO2008013919A2 (fr) 2006-07-27 2008-01-31 The Regents Of The University Of California Nanosondes de traçage de paroi latérale, leur procédé de fabrication et leur procédé d'utilisation
US8182783B2 (en) * 2006-11-16 2012-05-22 New Jersey Institute Of Technology Rapid microwave process for purification of nanocarbon preparations
US8478378B2 (en) 2007-09-04 2013-07-02 The Regents Of The University Of California Devices, systems and methods to detect endothelialization of implantable medical devices
CN101883545B (zh) * 2007-12-06 2013-08-07 纳诺西斯有限公司 可再吸收的纳米增强型止血结构和绷带材料
US20100229265A1 (en) 2008-03-26 2010-09-09 Sungho Jin Probe system comprising an electric-field-aligned probe tip and method for fabricating the same
US20130022494A1 (en) * 2008-06-26 2013-01-24 Exogenesis Corporation Method and system for sterilizing objects by the application of beam technology
WO2010003062A2 (fr) 2008-07-03 2010-01-07 The Regents Of The University Of California Matériaux biologiques et implants pour une formation améliorée de cartilage, et procédés de fabrication et d’utilisation de ceux-ci
WO2010022107A2 (fr) 2008-08-18 2010-02-25 The Regents Of The University Of California Revêtements nanostructurés superhydrophobes, superoléophobes et/ou superhomniphobes, procédés de fabrication et applications associés
US9539352B2 (en) * 2009-03-24 2017-01-10 Purdue Research Foundation Method and system for treating packaged products
EP2417637A4 (fr) 2009-04-09 2013-04-24 Univ California Cellules solaires à colorant en trois dimensions présentant des architectures nanométriques
US20110085968A1 (en) 2009-10-13 2011-04-14 The Regents Of The University Of California Articles comprising nano-materials for geometry-guided stem cell differentiation and enhanced bone growth
US9005648B2 (en) 2010-07-06 2015-04-14 The Regents Of The University Of California Inorganically surface-modified polymers and methods for making and using them
CN102348343A (zh) * 2010-08-03 2012-02-08 富泰华工业（深圳）有限公司 壳体及其制造方法
WO2012087352A2 (fr) 2010-12-20 2012-06-28 The Regents Of The University Of California Nanosurfaces super hydrophobes et super oléophobes
WO2013056186A1 (fr) 2011-10-12 2013-04-18 The Regents Of The University Of California Traitement de semi-conducteurs par gravure guidée par champ magnétique
JP6279488B2 (ja) 2012-02-07 2018-02-14 ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア タンタルでコーティングされたナノ構造を有する製品とその製作法および使用法
US20160071655A1 (en) 2013-04-04 2016-03-10 The Regents Of The University Of California Electrochemical solar cells
WO2014169281A1 (fr) * 2013-04-12 2014-10-16 Colorado State University Research Foundation Traitements de surface pour des endoprothèses vasculaires et procédés correspondants
WO2014172416A1 (fr) * 2013-04-17 2014-10-23 Tikekar Rohan Vijay Désinfection par ultraviolets de produits, liquides et surfaces
JP6622692B2 (ja) 2013-04-22 2019-12-18 ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア 切換可能な気体及び液体の放出及び送達デバイス、システム及び方法
WO2015074006A1 (fr) 2013-11-15 2015-05-21 The Regents Of The University Of California Dispositifs électrochimiques comprenant des électrolytes à base de solvant de type gaz comprimé
US9365427B2 (en) * 2014-03-07 2016-06-14 Industry-Academia Cooperation Group Of Sejong Univ Method for purifying carbon nanotubes
BR112016030273A2 (pt) * 2014-06-24 2017-08-22 Icon Medical Corp Dispositivo médico e método para formar o referido dispositivo
US20170243803A1 (en) * 2015-05-27 2017-08-24 Bridge Semiconductor Corporation Thermally enhanced semiconductor assembly with three dimensional integration and method of making the same
US20170138646A1 (en) 2015-10-12 2017-05-18 General Engineering & Research, L.L.C. Cooling device utilizing thermoelectric and magnetocaloric mechanisms for enhanced cooling applications
WO2017096044A1 (fr) 2015-12-01 2017-06-08 The Regents Of The University Of California Textiles adaptatifs intelligents, leur procédé de production, et leurs applications
WO2017132567A1 (fr) 2016-01-28 2017-08-03 Roswell Biotechnologies, Inc. Appareil de séquençage d'adn massivement parallèle
CA3027669A1 (fr) * 2016-06-21 2017-12-28 Medident Technologies Inc. Dispositif plasmaclave
US10451321B2 (en) 2016-09-02 2019-10-22 General Engineering & Research, L.L.C. Solid state cooling device
US20190376925A1 (en) 2016-11-22 2019-12-12 Roswell Biotechnologies, Inc. Nucleic acid sequencing device containing graphene
US10857575B2 (en) 2017-02-27 2020-12-08 Nanovation Partners LLC Shelf-life-improved nanostructured implant systems and methods
US10610621B2 (en) * 2017-03-21 2020-04-07 International Business Machines Corporation Antibacterial medical implant surface
US20190117827A1 (en) * 2017-10-25 2019-04-25 Mirus Llc Medical Devices

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020159917A1 (en) * 2001-04-27 2002-10-31 Swart Sally Kay System and method for cleaning, high level disinfection, or sterilization of medical or dental instruments or devices
US20020198601A1 (en) * 2001-06-21 2002-12-26 Syntheon, Llc Method for microporous surface modification of implantable metallic medical articles and implantable metallic medical articles having such modified surface
US20050252805A1 (en) * 2004-05-11 2005-11-17 Cervantes Marvin J Protective packaging assembly for medical devices and method of using same
WO2006043166A2 (fr) * 2004-10-22 2006-04-27 Guya Bioscience S.R.L. Procede de preparation d'implants intraosseux presentant un haut degre d'integration osseuse par formation d'une couche mince de dioxyde de titane de structure cristalline anatase
US20090250588A1 (en) * 2006-01-04 2009-10-08 Liquidia Technologies, Inc. Nanostructured Surfaces for Biomedical/Biomaterial Applications and Processes Thereof
US20110116967A1 (en) * 2007-11-21 2011-05-19 University Of Florida Research Foundation Inc. Self-sterilizing device using plasma fields
US20120288699A1 (en) * 2011-05-11 2012-11-15 Ahlberg Elisabet Biocompatible component
US20130323119A1 (en) * 2012-06-01 2013-12-05 Carefusion 303, Inc. System and method for disinfection of medical devices
US20170007743A1 (en) * 2014-03-26 2017-01-12 Nanovis, LLC Anti-microbial device and method for its manufacture

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MANDRACCI PIETRO ET AL.: "Surface Treatments and Functional Coatings for Biocompatibility Improvement and Bacterial Adhesion Reduction in Dental Implantology", COATINGS, vol. 6, no. 7, 2016, pages 2 - 22, XP055537056 *
PANKOVA E.A. ET AL.: "Investigation of the effect of HF-plasma on the chemical composition of collagen and keratin Containing HMM on the example of model compounds", 2012, pages 81 - 83 *

Also Published As

Publication number Publication date
US10857575B2 (en) 2020-12-08
US20180243803A1 (en) 2018-08-30

Similar Documents

Publication Publication Date Title
Liu et al. Nano-modified titanium implant materials: a way toward improved antibacterial properties
CN102732898B (zh) 在医用钛或钛合金表面制备微纳米复合结构的方法
Kizuki et al. Apatite-forming PEEK with TiO 2 surface layer coating
JP2004523291A (ja) 医療用インプラントの製造方法
US10857575B2 (en) Shelf-life-improved nanostructured implant systems and methods
KR101701264B1 (ko) 생체이식용 금속, 금속 제조방법, 이를 이용한 임플란트 및 스텐트
Motola et al. Thin TiO2 coatings by ALD enhance the cell growth on TiO2 nanotubular and flat substrates
CN110241451B (zh) 一种表面改性钛植入物及其功能化处理方法
JP2008080102A (ja) インプラント
JP2019511346A (ja) 組織接着性向上用コーティング
EP2156851B1 (fr) Procédé d'obtention d'un implant biocompatible
JP4635177B2 (ja) 生体親和性インプラント材及びその製造方法
US9889229B2 (en) Surface modification of implant devices
RU2554819C1 (ru) Способ получения биоактивного покрытия на имплантируемом в костную ткань человека титановом имплантате
KR100814355B1 (ko) 티타네이트 산화막 임플란트의 제조 방법 및 그 방법에의해 제조되는 티타네이트 산화막 임플란트
Henao et al. Study of HVOF-sprayed hydroxyapatite/titania graded coatings under in-vitro conditions
KR101696994B1 (ko) 다공성 이산화티타늄 나노입자 코팅층이 형성된 생체재료 및 이의 제조방법
Wu et al. Bioactivity of metallic biomaterials with anatase layers deposited in acidic titanium tetrafluoride solution
CN109045351A (zh) 一种基于表面处理的镁合金与丝素蛋白连接方法
Al-Swayih The electrochemical behavior of titanium improved by nanotubular oxide formed by anodization for biomaterial applications: A review
Rafieerad et al. Vertically oriented ZrO2TiO2Nb2O5Al2O3 mixed nanopatterned bioceramics on Ti6Al7Nb implant assessed by laser spallation technique
CN111020669A (zh) 一种医用钛金属表面S-TiO2-x薄膜的制备方法
Djendel et al. Improved corrosion and adhesion properties of titanium alloy for endoprostheses applications using a two-step anodization method
Gautam et al. Implant surface modification as a basis of osseointegration: A narrative review
CN114453593A (zh) 一种具有生物活性的个性化定制钛合金植入体支架的制备方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 18757642

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 18757642

Country of ref document: EP

Kind code of ref document: A1